CN101879603B - Production method and production device of tantalum powder - Google Patents
Production method and production device of tantalum powder Download PDFInfo
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- CN101879603B CN101879603B CN2010102041667A CN201010204166A CN101879603B CN 101879603 B CN101879603 B CN 101879603B CN 2010102041667 A CN2010102041667 A CN 2010102041667A CN 201010204166 A CN201010204166 A CN 201010204166A CN 101879603 B CN101879603 B CN 101879603B
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Abstract
The invention discloses a production device of tantalum powder, which comprises a reaction vessel and a reaction vessel cover, wherein the reaction vessel cover is hermetically sealed with the reaction vessel; the reaction vessel cover is provided with a plurality of through holes; a thermocouple, a stirring device and a sodium injecting tube are respectively arranged in the through holes; a feed inlet, a gas inlet and an exhaust port are also arranged on the reaction vessel cover; and the production device also comprises an alkali metal collector. The invention also discloses a method for producing the tantalum powder by utilizing the device. The tantalum powder prepared by the method of the invention has low content of oxygen, potassium and sodium, and the alkali metal collector is used for collecting the discharged alkali metal vapor, thereby reducing the pollution on the atmosphere, recycling alkali metals and reducing the production cost.
Description
Technical field
The present invention relates to the production method and the device of tantalum powder, particularly alkali metal reduction potassium floutaramite is produced the method for tantalum powder and is had the sodium reduction reaction unit of alkali metal gatherer.
Background technology
The powder of metal tantalum, the dense oxidation film that the powder surface generates has the valve metal character of unilateal conduction.The anode film stable chemical performance of processing (particularly in acidic electrolyte bath stable), resistivity high (7.5 * 1010 Ω cm), dielectric constant big (27.6), leakage current are little.Also have advantages such as operating temperature range wide (80～200 ℃), reliability height, antidetonation and long service life.
Alkali metal reduction potassium floutaramite is an important method of producing the tantalum powder, particularly produces the main method of high specific capacitance tantalum powder.Since inventing with the sodium reduction potassium floutaramite, He Lier Martin produces the tantalum powder to today, existing about 40 years history, and in order to obtain the purity height, the tantalum powder that specific area is big, people have paid many effort, and this has been proposed many improving one's methods.
The chemical equation of alkali metal reduction potassium floutaramite is:
K
2TaF
7+5Me＝Ta+2KF+5MeF
Me is an alkali metal in the following formula, like metallic potassium, sodium and their alloy, uses sodium metal usually.If use sodium metal reduction potassium floutaramite, its chemical equation is:
K
2TaF
7+5Na＝Ta+2KF+5NaF
In the process of actual production tantalum powder, in order to obtain more fine grain tantalum powder, in raw material, add diluent, like sodium chloride, potassium chloride, potassium fluoride and grain refiner etc.React the product that obtains, wrap up the coagula of tantalum powder for the melt of sodium chloride, potassium chloride, potassium fluoride and sodium fluoride.Usually with this coagula of pure water soaking and water washing, the tantalum powder is separated with sodium chloride, potassium chloride, potassium fluoride and sodium fluoride obtain the tantalum powder.
When the sodium reduction potassium floutaramite, if the sodium quantity not sufficient that adds will have the small amount of fluorine potassium tantalate not to be reduced, the yield of metal tantalum is low, and resulting like this tantalum powder oxygen content is high, and potassium, sodium content are also high.In order to make above-mentioned reacting completely, improve the yield of metal tantalum, often to excessively add sodium metal.
After the sodium reduction potassium floutaramite finished, superfluous alkali metal was that the form with sodium-potassium eutectic is present in the product.Past people is emitted part alkali metal with vapor form, mainly comprises sodium-potassium eutectic in the vapour of an alkali metal.Yet, also have a large amount of alkali metal to be present in the coagula.Under the situation that has water to exist, can produce tantalates and/or inclined to one side tantalates, chemical reaction is following:
Ta+Me+nH
2O＝MeTaO
3·nH
2O
When producing the tantalum powder, when having alkali metal in the product of sodium reduction potassium floutaramite, will form the tantalates that is insoluble in acid or be insoluble to sour inclined to one side tantalates.Particularly when producing the Ta powder used in capacitor of high-specific surface area, because the specific area of tantalum powder is big, in strong alkali solution; Produce a large amount of tantalates and/or inclined to one side tantalates; So just caused the loss of tantalum metal, and the oxygen content of tantalum powder and alkali metal content are high.The application of tantalum all requires high-purity, as making electrolytic capacitor anode, requires oxygen, potassium, sodium content low.
The toxic emission that contains vapour of an alkali metal pollutes environment in air.When the product of sodium reduction potassium floutaramite is stirred in washing, use a large amount of water, a large amount of waste water that contain alkali also can pollute environment.
Summary of the invention
In order to address the above problem, the present invention provides a kind of production method of tantalum powder, and it gets rid of alkali metal through negative pressure, and washing obtains the tantalum powder then.A kind of process units of tantalum powder also is provided accordingly.
For achieving the above object; The present invention adopts following technical scheme: a kind of process units of tantalum powder; Comprise reaction vessel and the reaction vessel lid that carries out hermetic seal with reaction vessel, reaction vessel covers and is provided with some through holes, is respectively equipped with thermocouple, agitating device and sodium injection tube in the through hole; Reaction vessel covers and also is provided with charge door, air inlet and exhaust outlet, and this process units also comprises the alkali metal gatherer.
Further, the exhaust outlet of said reaction vessel links to each other with the alkali metal gatherer, through the outside exhaust of alkali metal gatherer with find time.
Further; Said alkali metal gatherer comprise tank body and with the lid of tank body hermetic seal; Tank body top is provided with the alkali metal condenser that is used for the condensation vapour of an alkali metal, and the sidewall of tank body is provided with the but cooling jacket of medium turnover of cooling, and said alkali metal gatherer also comprises air inlet pipe and blast pipe; Said air inlet pipe one end links to each other with the exhaust outlet of reaction vessel; The other end runs through said lid straight cutting goes into the bottom of alkali metal gatherer, and said blast pipe one end runs through said lid, and the other end links to each other with evacuation system.
As one embodiment of the present invention, said alkali metal condenser is made up of the multilayer baffle plate, and the 1-6cm distance is arranged between plate and the plate, and every plate and inner tank wall have the slit of 1-10cm, and air inlet pipe runs through the bottom that baffle plate inserts tank body.
As one embodiment of the present invention, the alkali metal condenser is the porose metal basket in bottom, and the inside holds wire or metal fillings, and the slit of 1-10cm is arranged between basket and the inner tank wall.
A kind of method of utilizing said apparatus to produce the tantalum powder after the reaction of sodium reduction potassium floutaramite is accomplished, is got rid of alkali metal 600 ℃～900 ℃ negative pressure, and washing obtains the tantalum powder then.
Further, the reaction of sodium reduction potassium floutaramite vacuumized 0.5～2 hour at 600 ℃～900 ℃ after accomplishing, and was evacuated down to 500Pa～800Pa, and washing obtains the tantalum powder then.
Further, the exhaust outlet of reaction vessel links to each other with the alkali metal gatherer, through the outside exhaust of alkali metal gatherer with find time.
The present invention has following beneficial effect: oxygen, potassium, the sodium content of the tantalum powder that 1) makes according to the inventive method are low.2) collect the eliminating vapour of an alkali metal through the alkali metal gatherer, reduce pollution, recycle alkali metal, reduce production costs atmosphere.
Description of drawings
Fig. 1 is the structural representation of a kind of embodiment of tantalum powder process units of the present invention;
Fig. 2 is the structural representation of the another kind of embodiment of tantalum powder process units of the present invention.
The specific embodiment
Reach technological means and the effect that predetermined goal of the invention is taked for further setting forth the present invention; Below in conjunction with accompanying drawing and preferred embodiment; To the production method and the specific embodiment, characteristic and the effect of device of the tantalum powder that proposes according to the present invention, detailed description as follows.
As shown in Figure 1; Be that reaction unit of the present invention mainly comprises reaction vessel 1, reaction vessel lid 2, itself and reaction vessel hermetic seal; On reaction vessel lid 2, be provided with some through holes; Be respectively equipped with sodium injection tube 3, agitating device and thermocouple 5 in the through hole, said agitating device comprises puddler 41 and paddle 42, and driven by motor is used in puddler 41 upper ends.Near the center of reaction vessel lid 2, be provided with inflation inlet 7 and the charge pipe 6, the sodium injection tube 3 that are used to add potassium floutaramite, the marginal position that covers at reaction vessel is provided with exhaust outlet 8.The exhaust outlet 8 of said reaction vessel 1 links to each other with the alkali metal gatherer through air inlet pipe 96, through the outside exhaust of alkali metal gatherer with find time.Said alkali metal gatherer comprise tank body 91 and with the lid 92 of tank body hermetic seal; Tank body 91 tops are provided with the alkali metal condenser 93 of condensation vapour of an alkali metal; The bottom of tank body 91 holds alkali-metal zone for collecting, and the sidewall of tank body 91 is provided with the but cooling jacket of medium turnover of cooling, and the bottom of chuck is the import 94 of cooling medium; The top of chuck is the outlet 95 of cooling medium; Said alkali metal gatherer also comprises air inlet pipe 96 and blast pipe 97, and said air inlet pipe 96 1 ends link to each other with the exhaust outlet 8 of reaction vessel, and the other end runs through said lid 92 straight cuttings goes into the bottom of alkali metal gatherer; Said blast pipe 97 1 ends run through said lid, and the other end links to each other with evacuation system.
As shown in Figure 1, alkali metal condenser 93 is made up of the multilayer baffle plate, between plate and the plate certain distance is arranged, 1-6cm for example, and every plate and inner tank wall have the slit of 1-10cm, and air inlet pipe 96 runs through the bottom that baffle plate inserts tank body 91.Vapour of an alkali metal is condensed under the fluid drips through alkali metal condenser 93, collects in tank body 91 bottoms.
Another kind of embodiment as reaction unit of the present invention; As shown in Figure 2; Alkali metal condenser 93 ' be the porose metal basket in bottom, the inside holds wire or metal fillings, and the slit of 1-10cm is arranged between basket and the inner tank wall; Vapour of an alkali metal is collected in tank body 91 bottoms through alkali metal condenser 93 ' be condensed under the fluid drips.
In the sodium reduction process and in the insulating process after react, the air inlet pipe 96 of alkali metal gatherer is received the exhaust outlet 8 of reaction vessel 1, the mist that contains vapour of an alkali metal is discharged in the atmosphere after through the collection of alkali metal gatherer again.
After the sodium reduction reaction is accomplished, with the exhaust outlet connection vavuum pump of alkali metal gatherer, like mechanical pump, water ring pump.Can find time since 900 ℃, preferably found time 0.5～2 hour at 600 ℃～800 ℃, vacuum reaches 500pa～800pa.Find time and in the scope of a variations in temperature, to carry out.
The alkali metal gatherer can use in one or more series connection.
Embodiment 1
Use device as shown in Figure 1, the air inlet pipe 96 of alkali metal gatherer is received the exhaust outlet 8 of reaction vessel 1.The sodium chloride of the potassium floutaramite of 160kg and 100kg is packed in the reaction vessel 1, charge into argon gas after finding time, reaction vessel is hung in the electrothermal furnace 10, be warmed up to 900 ℃, stir, be incubated and begin to annotate sodium after 1 hour, inject the 49kg sodium metal altogether.Continue to stir insulation, send into argon gas from inflation inlet 7, from exhaust outlet 8 exhausts 20 minutes.Stop heating then and continue inflation, exhaust, when temperature in the reaction vessel drops to 800 ℃, the exhaust outlet connection vavuum pump of alkali metal gatherer is found time, found time 1 hour, then cool to room temperature.Solidification products in the reaction vessel is taken out, and broken after washing obtains tantalum powder 70.13kg, and the yield of tantalum is 95.0%.Collect alkali metal 1.12kg from the alkali metal gatherer, utilize again after the purification.Analyze oxygen, potassium, the sodium content of tantalum powder, data are listed in table 1.
Comparative example 1
Use existing reaction unit, the exhaust outlet of its reaction vessel directly leads to atmosphere.The sodium chloride of the potassium floutaramite of 160kg and 100kg is packed in the reaction vessel 1, charge into argon gas after finding time, reaction vessel is hung in the electrothermal furnace 10, be warmed up to 900 ℃, stir, be incubated and begin to annotate sodium after 1 hour, inject the 49kg sodium metal altogether.Continue to stir insulation, send into argon gas from inflation inlet 7, from exhaust outlet 8 exhausts 20 minutes.Stop heating then, cool to room temperature takes out product in reaction vessel, and broken after washing obtains tantalum powder 69.91kg, and the yield of tantalum is 94.71%.Analyze oxygen, potassium, the sodium content of tantalum powder, data are listed in table 1.
Embodiment 2
Use device as shown in Figure 2, the air inlet pipe 96 of alkali metal gatherer is received the exhaust outlet 8 of reaction vessel 1.100kg potassium chloride, 60kg sodium chloride and 40kg potassium fluoride are packed in the reaction vessel 1, charge into argon gas after finding time, reaction vessel is hung in the electrothermal furnace 10; Be warmed up to 850 ℃, stir, be incubated after 1 hour in the 30kg potassium floutaramite adding reaction vessel 1; Begin to annotate sodium and continue and stir; Divide then 3 times, add the 20kg potassium floutaramite at every turn, begin to annotate sodium behind the adding potassium floutaramite.Add potassium floutaramite 90kg altogether, inject sodium metal 27.6kg.Continue to stir insulation, send into argon gas from inflation inlet 7, from exhaust outlet 8 exhausts 20 minutes.Stop heating then and continue inflation, exhaust, when temperature in the reaction vessel drops to 600 ℃, the exhaust outlet connection vavuum pump of alkali metal gatherer is found time; Find time to be incubated 30 minutes; Cool to room temperature takes out product in reaction vessel then, broken after washing; Obtain tantalum powder 38.20kg, the yield of tantalum is 92.00%.Analyze oxygen, potassium, the sodium content of tantalum powder, data are listed in table 1.
Comparative example 2
Use existing reaction unit, the exhaust outlet of its reaction vessel directly leads to atmosphere.100kg potassium chloride, 60kg sodium chloride and 40kg potassium fluoride are packed in the reaction vessel 1, charge into argon gas after finding time, reaction vessel is hung in the electrothermal furnace 10; Be warmed up to 850 ℃, stir, after the insulation 1 as a child the 30kg potassium floutaramite is added in the reaction vessel 1; Begin to annotate sodium and continue and stir; Divide then 3 times, add the 20kg potassium floutaramite at every turn, begin to annotate sodium behind the adding potassium floutaramite.Add potassium floutaramite 90kg altogether, inject sodium metal 27.6kg.Continue to stir insulation, send into argon gas from inflation inlet 7, from exhaust outlet 8 exhausts 20 minutes.Stop to heat cool to room temperature then, product is taken out in reaction vessel, broken after washing obtains tantalum powder 37.72kg, and the yield of tantalum is 90.83%.Analyze oxygen, potassium, the sodium content of tantalum powder, data are listed in table 1.
Oxygen, potassium, sodium content (ppm) in the table 1 tantalum powder
| ? | O | K | Na |
| Embodiment 1 | 2000 | 4 | 4 |
| Comparative example 1 | 2500 | 13 | 10 |
| Embodiment 2 | 3600 | 9 | 4 |
| Comparative example 2 | 4100 | 18 | 7 |
Can find out from the data of table 1, the tantalum powder that uses method and apparatus of the present invention to obtain, its oxygen, potassium, sodium content are lower.
In this manual, the ppm of unit is meant " 1,000,000/" represented with mass ratio.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limiting the present invention, anyly be familiar with the professional and technical personnel, in not breaking away from technical scheme scope of the present invention; When the technology contents of above-mentioned announcement capable of using is made a little change or is modified to the equivalent embodiment of equivalent variations; In every case be not break away from technical scheme content of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (7)
1. the process units of a tantalum powder comprises reaction vessel and the reaction vessel lid that carries out hermetic seal with reaction vessel, and reaction vessel covers and is provided with some through holes; Be respectively equipped with thermocouple, agitating device and sodium injection tube in the through hole; Reaction vessel covers and also is provided with charge door, air inlet and exhaust outlet, it is characterized in that, this process units also comprises the alkali metal gatherer; Said alkali metal gatherer comprise tank body and with the lid of tank body hermetic seal; Tank body top is provided with the alkali metal condenser that is used for the condensation vapour of an alkali metal, and the sidewall of tank body is provided with the but cooling jacket of medium turnover of cooling, and said alkali metal gatherer also comprises air inlet pipe and blast pipe; Said air inlet pipe one end links to each other with the exhaust outlet of reaction vessel; The other end runs through said lid straight cutting goes into the bottom of alkali metal gatherer, and said blast pipe one end runs through said lid, and the other end links to each other with evacuation system.
2. a device as claimed in claim 1 is characterized in that, the exhaust outlet of said reaction vessel links to each other with the alkali metal gatherer, through the outside exhaust of alkali metal gatherer with find time.
3. a device as claimed in claim 1 is characterized in that, said alkali metal condenser is made up of the multilayer baffle plate, and the 1-6cm distance is arranged between plate and the plate, and every plate and inner tank wall have the slit of 1-10cm, and air inlet pipe runs through the bottom that baffle plate inserts tank body.
4. a device as claimed in claim 1 is characterized in that, the alkali metal condenser is the porose metal basket in bottom, and the inside holds wire or metal fillings, and the slit of 1-10cm is arranged between basket and the inner tank wall.
5. the method for producing the tantalum powder is installed in a utilization according to claim 1, it is characterized in that, after the reaction of sodium reduction potassium floutaramite is accomplished, gets rid of alkali metal 600 ℃～900 ℃ negative pressure, and washing obtains the tantalum powder then.
6. a method as claimed in claim 5 is characterized in that, the reaction of sodium reduction potassium floutaramite vacuumized 0.5～2 hour at 600 ℃～900 ℃ after accomplishing, and was evacuated down to 500Pa～800Pa, and washing obtains the tantalum powder then.
7. a method as claimed in claim 5 is characterized in that, the exhaust outlet of reaction vessel links to each other with the alkali metal gatherer, through the outside exhaust of alkali metal gatherer with find time.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102191389B (en) * | 2011-04-19 | 2013-09-25 | 潘伦桃 | Rinsing method of potassium fluotantalate product obtained through sodium reduction |
| CN102380619A (en) * | 2011-10-10 | 2012-03-21 | 肇庆多罗山蓝宝石稀有金属有限公司 | Method for reducing impurity content in tantalum powder produced by sodium reducing method |
| US9260765B2 (en) * | 2013-03-15 | 2016-02-16 | Ati Properties, Inc. | Process for producing tantalum alloys |
| US9994929B2 (en) | 2013-03-15 | 2018-06-12 | Ati Properties Llc | Processes for producing tantalum alloys and niobium alloys |
| CN104801725B (en) * | 2015-05-18 | 2018-01-23 | 江门富祥电子材料有限公司 | A kind of reaction unit of sodium reduction potassium floutaramite and manufacture the method for tantalum powder with it |
| CN106862579A (en) * | 2016-12-28 | 2017-06-20 | 芜湖顺景自动化设备有限公司 | A kind of sodium reduction device with insulating |
| CN108080654B (en) * | 2018-01-23 | 2019-01-08 | 江门富祥电子材料有限公司 | A kind of production technology of ultra-fine flake type mesohigh tantalum powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2950185A (en) * | 1958-06-13 | 1960-08-23 | Nat Res Corp | Production of tantalum powder |
| US5442978A (en) * | 1994-05-19 | 1995-08-22 | H. C. Starck, Inc. | Tantalum production via a reduction of K2TAF7, with diluent salt, with reducing agent provided in a fast series of slug additions |
| CN201693182U (en) * | 2010-06-18 | 2011-01-05 | 江门富祥电子材料有限公司 | Production device for tantalum powder |
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| WO2007130483A2 (en) * | 2006-05-05 | 2007-11-15 | Cabot Corporation | Tantalum powder with smooth surface and methods of manufacturing same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2950185A (en) * | 1958-06-13 | 1960-08-23 | Nat Res Corp | Production of tantalum powder |
| US5442978A (en) * | 1994-05-19 | 1995-08-22 | H. C. Starck, Inc. | Tantalum production via a reduction of K2TAF7, with diluent salt, with reducing agent provided in a fast series of slug additions |
| CN201693182U (en) * | 2010-06-18 | 2011-01-05 | 江门富祥电子材料有限公司 | Production device for tantalum powder |
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